Trimethyl phosphite → HCID 53693742, Verbindung

HRID 487888Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 487888
Br[CH2:2][C:3]1[C:12]([CH2:13]Br)=[CH:11][C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[CH:4]=1.C[O:16][P:17]([O:20][CH3:21])[O:18][CH3:19]>C1(C)C=CC=CC=1>[CH3:19][O:18][P:17]([CH2:2][C:3]1[C:12]([CH2:13][P:17](=[O:16])([O:20][CH3:21])[O:18][CH3:19])=[CH:11][C:10]2[C:5]([CH:4]=1)=[CH:6][CH:7]=[CH:8][CH:9]=2)(=[O:16])[O:20][CH3:21]

Komponenten

4

Edukt 2

HCID 8472Trimethyl phosphiteHCID 2622592,3-Bis(bromomethyl)naphthalene

Produkt 1

HCID 53693742HCID 53693742, VerbindungAusbeute 97,8 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1140TolueneLösungsmittel

Versuchsvorschrift

A flask is charged with 2,3-bis(bromomethyl)naphthalene (Example 22(b), 2.80 g, 8.9 mmol) and toluene (50 mL). The solution is heated at reflux and 25 mL of the toluene is collected in a Dean-Stark trap. The solution is then cooled to room temperature and trimethylphosphite (4.0 mL, 0.034 mol) is added. The reaction is heated to reflux temperature for 24 hours. The excess trimethylphosphite and toluene are removed at reduced pressure, giving a white solid (3.24 g). The solid is recrystallized from ethyl acetate-hexane to give 2.55 g of white crystals, mp 119.5°-120.5° C.

Aufarbeitung

  1. temperatureThe solution is heated
  2. temperatureat reflux
  3. custom25 mL of the toluene is collected in a Dean-Stark trap
  4. temperatureThe reaction is heated
  5. temperatureto reflux temperature for 24 hours
  6. customThe excess trimethylphosphite and toluene are removed at reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-b6ff4fede09d45659eea1b973a38a3ba
Quelldatensatz
uspto-grants-1994_03
Patentnummer
US05298498

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